ASTM D5176-91(1995)

Standard Test Method for Total Chemically Bound Nitrogen in Water by Pyrolysis and Chemiluminescence Detection

SCOPE
1.1 This test method covers the determination of the total nitrogen content of water in concentrations from 0.5 to 1000 mg/L. Higher nitrogen concentrations may be determined by making the proper dilutions.
1.2 This test method does not determine molecular nitrogen (N2).
1.3 The values stated in SI units are to be regarded as the standard.
1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Dec-1994
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaced By: ASTM D5176-91(2003) - Standard Test Method for Total Chemically Bound Nitrogen in Water by Pyrolysis and Chemiluminescence Detection
• Effective Date: 10-Mar-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact
ASTM International (www.astm.org) for the latest information.
Designation: D 5176 – 91 (Reapproved 1995)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Total Chemically Bound Nitrogen in Water by Pyrolysis and
Chemiluminescence Detection
This standard is issued under the fixed designation D 5176; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Significance and Use
1.1 This test method covers the determination of the total 5.1 This test method is useful for the determination of total
nitrogen content of water in concentrations from 0.5 to 1000
chemically bound nitrogen in wastewaters and other waters.
mg/L. Higher nitrogen concentrations may be determined by
making the proper dilutions. 6. Apparatus
1.2 This test method does not determine molecular nitrogen
6.1 Pyrolysis Furnace—An electric tube furnace capable of
(N ).
achieving a temperature of 1100°C. The furnace may be single
1.3 The values stated in SI units are to be regarded as the
or multizoned and may have common or separate and inde-
standard. The values given in parentheses are for information
pendent temperature controls.
only.
6.2 Pyrolysis Tube—The pyrolysis tube must be fabricated
1.4 This standard does not purport to address all of the
from quartz and should be designed to ensure complete
safety concerns, if any, associated with its use. It is the
pyrolysis of a wide variety of samples.
responsibility of the user of this standard to establish appro-
6.3 Chemiluminescence Detector—The detector shall have
priate safety and health practices and determine the applica-
a photomultiplier tube capable of sensing the light emission of
bility of regulatory limitations prior to use.
the decaying NO *. The detector shall have digital display,
onboard ozone generator and analog output for data system or
2. Referenced Documents
strip chart recorder.
2.1 ASTM Standards:
6.4 Recorder (optional)—The recorder shall be able to
D 1129 Terminology Relating to Water
2 accept a 1 V full scale signal and to provide a chart speed of 1
D 1193 Specification for Reagent Water
cm/min.
D 2777 Practice for Determination of Precision and Bias of
6.5 Microlitre Syringe—Any standard series of microlitre
Applicable Methods of Committee D-19 on Water
syringes with stainless steel needles is acceptable. See manu-
3. Terminology
facturer’s instructions for appropriate syringe sizes.
3.1 Definitions—For definitions of terms used in this test 6.6 Syringe Drive Mechanism—The syringe drive shall be
method, refer to Terminology D 1129.
capable of driving the sample from a microlitre syringe at a
3.2 Definition of Term Specific to This Standard: controlled, reproducible rate.
3.2.1 total chemically bound nitrogen—all inorganic and
6.7 Sample Boat—Samples with high concentrations of
organic nitrogen in the sample, except molecular nitrogen (N ).
suspended matter or dissolved nonvolatile compounds may
tend to plug the syringe needle upon injection into the pyrolysis
4. Summary of Test Method
tube. In this case a sample boat of quartz or platinum, with or
4.1 The sample of water is introduced into a stream of
without quartz wool, should be used, in conjunction with the
oxygen or inert/oxygen mix flowing through a quartz pyrolysis
appropriate pyrolysis tube. The pyrolysis tube shall allow the
tube. Oxidative pyrolysis converts chemically bound nitrogen
introduction of the sample into the boat by microlitre syringe
to nitric oxide (NO). The gas stream is dried and the NO is
without interrupting the gas flow system.
contacted with ozone (O ) producing metastable nitrogen
dioxide (NO *). As the NO * decays, light is emitted and
2 2 7. Reagents and Materials
detected by a photomultiplier tube. The resulting signal is a
7.1 Purity of Reagents—Reagent grade chemicals shall be
measure of the total chemically bound nitrogen in the sample.
used. Unless otherwise indicated, it is intended that all reagents
shall conform to the specifications of the Committee on
This test method is under the jurisdiction of ASTM Committee D-19 on Water
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water. The apparatus described in 6.1-6.7 is manufactured by Antek Instruments, Inc.,
Current edition approved Sept. 15, 1991. Published February 1992. Houston, TX and Dohrmann Division of Rosemount Analytical Inc., Santa Clara,
Annual Book of ASTM Standards, Vol 11.01. CA, and was used in the validation study of this test method.
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 5176
Analytical Reagents of the American Chemical Society. each determination, the only variables will be total nitrogen
Other grades may be used, provided it is first determined that concentration and detector response (digital display). Construct
the reagent is of sufficiently high purity to permit its use a curve plotting milligrams of N per litre versus detector
without lessening the accuracy of the determination. response. Check the complete calibration curve at least once
7.2 Purity of Water—Unless otherwise indicated, references per week; check one or two standards daily.
to water shall be understood to mean reagent water conforming
10. Procedure
to Specification D 1193, Type I.
10.1 Flush the microlitre syringe several times with the
7.3 Inert Gas, Argon (minimum purity 99.99 %).
7.4 Oxygen (minimum purity 99.6 %). unknown sample. Inject the sample at a controlled rate of 1 to
2 μg/s as described in 9.3 or inject the sample into the sample
7.5 Stock Solution, Pyridine (10 000 mg N/L)—Prepare by
accurately weighing 5.647 g of pyridine into a 100 mL boat (see 6.7) as described in 9.4.
10.2 Set instrument parameters as recommended by manu-
volumetric flask and dilute to 100 mL with water.
7.6 Pyridine Solutions, Standard (1000, 500, 100, 50, 10, 5, facturers. Some changes may be needed to accommodate
specific kinds of samples.
1, and 0.5 mg N/L)—Dilute ten volumes of the stock solution
(see 6.5) with 90 volumes of water to prepare a 1000 mg N/L
11. Calculation
standard. Simi
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